Treating apparatus



C.v E. BURKE AND G. BARNHART.

. TREATING APPARATUS.` APPLICATION FILED APK. 27. I92o.

atented D. 6, 1921.

CHARLES E. BURKE, or -cAENEYs POINT, AND GEORGE BARNHART, 0F WOODSTOWN,

NEW JERSEY, ASSIGNORS TO E. I. DU PONT DE NEMOURS & COMPANY, 0F WILMING- TON, DELAWARE, A CORPORATION 0F DELAWARE.

TREATING APPARATUS.

Specification of Letters Patent.

Patented Dec. 6, T921.

Application led April 27, 192.9. SerialN'o. 377,060.

To all whom it may con-cern.'

Be it known that we, CHARLES E. BURKE and GEORGE BARNHART, citizens of the Dominion of Canada and the United States, respectively, and residents of Carneys Point, county of Salem, and State of New Jersey,

`and Woodstown, county of Salem, and State of New Jersey, respectively. have invented a certainl new and useful Treating Apparatus, of which the following is a specification.

This invention relates to apparatus for chemically treating materials, and more particularly to apparatus by the aid of which the material in question may be continuously treated, the present apparatus providing for the uninterrupted passage of the material therethrough, the constant supplying of the chemical necessary for the treatment desired, and the proper handling of the material and chemical lwhile in the apparatus. The invention ,finds particularly advantageous application when embodied in nitration apparatus and, specifically, when embodied in apparatus for the nitration of oil, and therefore we describe it with more 'particular reference to the art of nitration; but, itwill be understood that we do not restrict it thereto, nor to the illustrated embodiment.

In nitrating, as usually practised, the material to be treated is treated in batches in a vessel of relatively large capacity, the nitrating acid being gradually added to the material, or vice versa, until an entire batch has been treated, andv after the nitration is completed the entire batch held in the nitrator is separatedpr drowned. A great difficulty with this metho`d is that the yearliertreated portions of the batch, although their treatment is completed, are allowed to remain in the vessel, and, so, are kept in contact with the strong acid, and so forth, until the treatment of the later-treated portions A is completed; the result is that the earliertreated portions suffer decomposition and are of inferior quality. Another difficulty is that the procedure entails frequent interruptions, with consequent loss of time and so forth; therefore to so far as possible` reduce the number of interruptions, it has been the practice, as mentioned above, to use a vessel of relatively large capacity in order to treat a relatively large quantity of material before having to interrupt the work and empty the vessel. This latter practice is, however, dangerous as in case of accident the large amount of material in the vessel is a great menace. The apparatus of the present invention eliminates these difliculties since it provides for the removal of the material immediately upon the' completion of its treatment; it is of small capacity so that the amount of material that would be involved in any accident is reduced to a minimum; and it provides for the uninterrupted -treatment of an unlimited quantity of material. An object ofthe invention is to provide an apparatus for the continuous treatment of material, and more specifically it is to iprovide an apparatus for continuous nitraion.

To this end, and also to improve generally upon apparatus of the character indicated, the invention consists in the various matters hereinafter described and claimed.

In the accompanying drawings Figure l is a diametrical section of an apparatus embodying the'invention, taken substantially on the line 1-1 of Fig. 2;

Fig. 2 is a plan view of the apparatus illustrated in Fig. l: Fig. 3 is an elevational view, with a portion of the outer wall of the container broken out, and portions of the inner walls sectioned, to show the interior construction, of an apparatus essentially similar t o the apparatus shown in Fig. l, but having modified feeding means; i

Fig. 4 is a plan view-of the apparatus illustrated in Fig. 3, and

Fig. 5-is an elevational view of the agitator, with the feeding means arranged as in the apparatus illustrated in Fig. 3.

Referring now to the drawings; and more particularly to Figs. 'l and 2:-

The container, designated generally as 1, comprises a preferably annular closed-bottom receptacle 2, within which is placed a second annular closed-bottom receptacle 3, extending substantially to the bottom of the receptacle 2, of relatively small capacity, and having its walls spaced all about from the Walls of the receptacle 2. The inner receptacle provides a reaction receptacle, or nitrating compartment, and the` outer receptacle constitutes' a chamber for a temperature controlling medium, for example cold brine. A pipe 4 entering the bottom of the receptacle 2 provides for the fiow of brine into, or out of, the receptacle, as de.- sired, while pipes 5 and 6 opening into the receptacle 2 adjacent its top, and communicating with the divisions 2a and 2b on opposite sides of the receptacle 3, provide for the flow of brine 'out of, or into, the receptacle 2, these pipes 4, 5 and 6 being desirably used for connection in circuit with any suitable brine-cooling means, as a cooling coil (not. shown). By making the inner receptacle of annular form, it will be seen that we conveniently provide the large wall area desirable for efficient-cooling, even though the inner receptacle is, as desired, of small capacity; also we provide for the use of a` vide a hydrostatic head sufficient to insure that the receptacle 3 can, if desired, be substantially completely filled with liquid. In this way it is provided that the oil and acid shall enter at the bottom of the receptacle and travel upward, Athe nitration taking place during the travel. A discharge pipe, as 9, communicating with the receptacle 3 above the inlets 7 and 8 is provided for the outflow of the nitrated oil.

Preferably a vertical series of pipes, as

9, 10 and 11, with the pipes at increasingheights, respectively, is provided, each pipe 9 or 10 having a valve as 9a or 10a for closing it when it is deslred that discharge occur from a higher pipe.v This' arrangement permits the ready determining of the time that any particular oil shall remain in the apparatus. That is, oils which are readily nitrated can be drawn from the lowest pipe, while by drawing a more-difficultly nitrated oil from a higher pipe the.. time during which that oil is under treatment can be made greater than that for a more easily nitrated oil.

The driven agitator, designated generally as 12, is preferably in the general character of a cylinder, being shown as of the basket type and comprising a suitable number, as twelve, or vertical members 13 extending substantially to the bottom of the receptacle 3, and connected together at their bottoms by a ring 14 and at their tops by a spider 15. The spider 15 serves as a convenient means for mounting the agitator upon la central shaft 16` to rotate therewith; the latter may be driven by any suitable means, for example the driving pulley 17, and may be supportedin any sultable way, as by radial-and-thrust bearings 18 and 19 supported, respectively, by the base 2O and the container 1. p

Conveniently, the inner receptacle 2 is supported from the outer Nreceptacle by' carrying the edges of the walls of one of the receptacles over to the adjacent edges of the walls of the other, as indicated at- 21 and 22, and .connecting them thereto, thus not only supporting the inner receptacle but also closing the top of the outer receptacle.

In operation, the materials, as oil and nitric acid, are fed to the apparatus as required, this bein conveniently done by any desired device not shown) for automatically measuring the oil and acid and discharging them into the pipes 7 and 8, the f agitator is rotated meanwhile at the' speed desirable for the particular treatment, and the nitrated oil is continuously drawn off by the particular pipe 9, 10-or 11, corresponding to the desired time of treatment; in the meantime the receptacle 2 is filled with brine and brine circulated therethrough as required. 4

The structure illustrated in Figs. 3, 4 and 5, while essentially like that shownin Figs. 1 and 2, has provisions particularly adapting it for use when unusually intimate mixing of the oil and acid is called for. In this apparatus, the oil and acid pipes, as 7 a and 8a, instead-of ibeing stationary, are carriedl by the agitator blades; thus, when the agitator rotates the pipes rotate therewith and the oil and acid are distributed along the path of rotation. Thepi'pes 7a and 8a eX- tend substantially t'o the lower end of the agitator and so, like the pipes 7 and 8, communicate with the receptacle 3 at its lower portion and, for practical purposes, at its v bottom. Their upper ends are carried radially inward to place Vthem over the 'center of rotation and thus permit their easy filling despite the rotation; as shown, one pipe, as 8a, is carried fluid tight u through the funnel-like end 7b of the ot er so that, if desired, suitable feed pipes (not shown) can be readily led to the end 7b and to the similar funnel-like end 8", without interference.

Any structural materials, suited to the particularmaterials to be handled, may be used in the construction of the apparatus, for working with oil and nitric acid we have found cast or wrought iron satisfactory.

We claim 1. In a continuous treating apparatus, in combination, an outer` -receptacle providing a chamber for a temperature-controlling medium, an inner reaction receptacle in the outer receptacle and spaced therefrom, means for introducing reacting materials 'receptacle at -therealong and both of into the inner receptacle and comprising a pair of reacting-material-introduction conduits, and means for withdrawing reaction products from such receptacle, said two means, with respect to each other, communicating with the inner receptacle at points spaced therealong, and the said conduits of said introducing means both being spaced from said withdrawing means in the same direction longitudinally of said reaction receptacle, whereby a pair of reacting materials can enter by said conduits and flow together along such receptacle toward said withdrawing means. 't

2. In a treating apparatus2 in combination, van outer receptacle providing a chamber for a temperature-controlling medium, an inner reaction receptacle in the outer receptacle and .spaced at its sides from the sides of the outer receptacle to provide two chamber divisions, means for conducting a temperature controlling medium to the outer receptacle, and means for conducting such medium from such receptacle, said two conducting means communicating with the outer points spaced therealong and at least one of such means being arranged, relative to said two chamber divisions, for ls)ubstantially immediate communication with oth.

l 3. In a treating apparatus, in combination, an outer receptacle providing a chamber for a temperature-controlling medium, an inner reaction receptacle in the outer receptacle and spaced atr its sides from the sides of the outer receptacle to provide two chamber divisions, means for conducting a temperature controlling medium to the outer receptacle, and means for conducting such medium from such receptacle, saidvtwo conducting means communicating with the outer receptacle at points spaced therealong and both of such means being arranged, relative to said two chamber divisions, for substantially immediate communication with both said divisions.

4. In a continuous treating apparatus, in combination, an outer receptacle providing a chamber for a temperature-controlling medium, an inner reaction rece tacle in the outer receptacle and spaced at its sides from the sides ofthe outer receptacle to provide two chamber divisions, means for introducing reacting materials to the inner receptacle and means for withdrawing reaction products from such receptacle, such two means, relative to each other, being' spaced along such receptacle to provide for4 continuous flow along the same, means for conducting a temperature controlling medium to the outer receptacle, and means for conducting such medium from such receptacle, said two conducting means communicating with the outer receptacle at points spaced such means being arranged, relative to said two chamber divisions, for substantially immediate communication with both said divisions.

5. In a continuous treating apparatus, in combination, a reaction receptacle adapted to be vertically arranged, means for introducing reacting materials to the receptacle and comprising a pair of reaction-materialintroduction conduits separately communicating with the receptacle at its lower portion, and means for withdrawing reaction products from the receptacle and communicating with the receptacle at its upper portion and above and spaced from the communication points of said conduits, whereby a pair of reacting materials can separately enter by said conduits and flow upward together in said receptacle toward said withdrawing means, and the' reaction product be withdrawn at said withdrawing means.

6. In a continuous treating apparatus, in combination, a reaction receptacle, means for introducing reacting materials to the receptacle and comprising a pair of reactingmaterial-introduction conduits, and -means for withdrawing reaction products from the receptacle, said two means, with respect to each other, communicating with the receptacle at points spaced therealong, and the said conduits lof said introducing means both being spaced from said withdrawing vmeans in the same direction longitudinally of said reaction receptacle, whereby a pair of reactin materials can enter by said conduits and gow together along such receptacle tosaid withdrawing means, and said withdrawing means comprising a plurality of optionally usable exits spaced from each .other along the receptacle thereby to serve as a means for controlling the time during which the reacting materials and the product shall remain in said reaction receptacle. 7. ln a continuous treating apparatus, in combination, a reaction receptacle adapted to be vertically arranged, means for introducingreacting materials to the receptacle adjacent the lower end thereof and comprising a pair of reacting-material-introduction conduits, and a plurality of devices adjacent the upper end of the receptacle for withdrawing reaction productsv from said receptacle vand spaced along said receptacle from said means, the units of said plurality being vertically spaced from each other and certain of them including Y provisions for optional closing and opening thereof whereby said plurality of exits serves as 'a means for controlling the time during which the reacting materials and the product shall remain in said reaction receptacle.

8. In a continuous treating apparatus, in combination, an outer receptacle providing a chamber for a temperature-controlling meouter receptacle and spaced at its sides from the sides of the outer .receptacle to'provide two chamberf divisions for the medium, means for conducting such medium to the outer receptacle and means for conducting such medium from such receptacle, said two means communicating with the outer receptacle at points spaced therealong and at least one of such means being arranged, relative to said chamber divisions, forsubstantially immediate communication with both, means for introducing reacting materials to the inner receptacle, and means for withdrawing reaction products from such receptacle, respect to each other, communicating with the inner receptacle at points spaced therealong, then said withdrawing means comprising a plurality of exits spaced from each other along the inner receptacle, with certain of said exists including provisions for optional closing and opening thereof.

9. In a continuous treating apparatus, in combination, a reaction receptacle adapted to be vertically arranged, means for introducing reacting materials to the receptacle comprising a pair of reacting-material-introduction conduits and discharging into the receptacle at its lower portion, and means for withdrawing reaction products from the receptacle and discharging therefrom adjacent its top portion, said introducing means including a device in the character of a vertically arranged pipe providing one of said conduits and of sufficient height to provide a hydrostatic head corresponding to the height of said withdrawing means above the said lower portion of the receptacle.

10. In a continuous treating apparatus, in combination, a` reaction receptacle adapted to be vertically arranged, means for introducing reaction materials to the receptacle and comprising a pair of reacting-materialintroduction conduits discharging into the receptacle at its lower portion, and means for withdrawing reaction products from the receptacle and discharging therefrom adjacent its top portion, sald introducing means including a pair of devices each in the character of a vertilly arranged pipe providing a respective one of said conduits and of sufficient height to provide a hydrostatic head corresponding to the height of said withdrawing means above the said lower portion.

11. In a treating apparatus, in combination, a reaction receptacle, a rotatable agitator therein, and a pair of devices for in troducing reacting materials to the receptacle and carried with said agitator to rotate therewith, said devices being separate and non-communicating whereby a pair of reacting materials may be separately and simultaneously introduced into said receptacle.

12. In a treating apparatus, in combination, a reaction receptacle, a rotatable agisaid latter named two means, with tator therein, and a pair of devices for introducing reacting materials to the receptacle, each of said devices being in the character of a pipe and each such pipe being mounted on said agitator to rotate therewith upon the axis thereof and having its receiving end in longitudinal alinement with such axis, one of said pipes, adjacent its receiving end, passing through the receiving end of the other.

13. In a treating apparatus, in combination, a reaction receptacle, a rotatable agitator therein, and a pair of devices for introducing reacting materials to the receptacle, each of said devices being in the character of a pipe and each such pipe being mounted on said agitator to rotate therewith upon the axis. thereof and having its receiving end in longitudinal alinement with such axis, one of said pipes, adjacent its receiving end, passing through the receiving end of the other, and said pipes being separate and non-communicating whereby a pair of reacting materials may be separately and simultaneously introduced into said receptacle.

14. In a continuous treating apparatus, in combination, an outer receptacle for a temperature-controlling medium, an inner receptacle in the outer receptacle, spaced from the side walls thereof to divide the outer receptacle into innerv and outer compartments, and extending to adjacent the bottom of the outer receptacle, means for circulating a temperaturecontrolling medium through said outer receptacle substantially throughout the length thereof and into and out of both its compartments, a pair of pipes for introducing reacting materials to the reaction receptacle, and a discharge device for withdrawing reaction products from the reaction receptacle, the discharge ends of said pair of pipes, and said discharge device, being spaced from each other longitudinally of said inner receptacle. y

15. In a continuous treating apparatus, 1n combination, an outer receptacle for a temperature-controlling medium, an annular inner receptacle in the outer receptacle, spaced from the side walls thereof to divide the outer receptacle into inner and outer compartments, and extending to adjacent the bottom of the outer receptacle, means for circulating a temperature-controlling medium through said outer receptacle substantially throughout the length thereof and into and out of both its compartments, a pair of pipes for introducing reacting materials to the reaction receptacle, and a discharge device for withdrawing reaction products -from the reaction receptacle, the discharge ends of said pair of pipes, and said discharge device, being spaced from each other longitudinally of said inner receptacle.

16. In a continuous treating apparatus, in combination, an outer receptacle for a temv circulating a temperature-controlling me.

perature-controlling medium, an annular inner receptacle in the outer receptacle, spaced from the side walls-thereof to divide the outer receptacle into inner and outer compartments, and extending to adjacent the bottom of the outer receptacle, means for dium through said outer receptacle substantially throughout the length thereof and into and out of both its compartments, a pair of pipes for introducing reacting materials to the reaction receptacle, a discharge device for withdrawing reaction products from the reaction receptacle, the dischargeends of said pair of pipes, and said discharge device, being spaced from each other longitudinally of said inner receptacle, and an agitator in said reaction receptacle mounted for rotation concentrically therewith, and extending substantially the length thereof.

In a continuous treating apparatus, in combination, an outer receptacle adapted to be vertically arranged and for a temperature-controlling medium, an annular inner reaction receptacle in the outer spaced from the'walls thereof to divide the outer receptacle into inner and outer compartments, and extending to adjacent the bottom of the outer receptacle, means for circulating a temperature-controlling mereceptacle,

dium through said outer receptacle'substantially throughout the length thereof and into and out of both its compartments, a pair of pipes for introdcin reacting materials to the reaction receptaca, and having their discharge orices such receptacle, a discharge device for withdrawing reaction products from the reaction at the bottom portion of receptacle and communicating therewith at t e upper portion thereof, and an agitator in said reaction receptacle, mounted forrotation `-concentrically therewith, and extending substantially the length thereof.

In a continuous treating apparatus, in combination, an outer receptacle adapted to be vertically arranged and for a temperature-controlling medium, an annular inner reaction receptacle in the outer receptacle, spaced all about from the walls thereof to divide the outer' receptacle into inner and outer compartments, and extending to adjacent the bottom of'the outer receptacle, means for circulating a temperature-controlling medium through said outer receptacle substantially throughout the length thereof and into and out `of both its compartments, a pair of pipes for introducing reacting materials to the reaction receptacle and having their discharge orifices at the lower portion of such receptacle, a discharge device for withdrawing reaction products from the rea actlon receptacle .and communicating therewith at the upperlportion thereof, and an agitator in said reaction receptacle, mount- CHARLES E. BURKE. GEORGE BARNHART. 

